EPSRC National Crystallography Service
Data Collection Summary kccd2 (damien)

Summary report for Directory: diska/2009src0115

Report generated Feb 06, 2009; 13:52:30

Unit cell

38165 reflections with 2.91°<theta<27.48° (resolution between 7.00A and 0.77A) were used for unit cell refinement

Symmetry used
in scalepack		p1
a (Angstrom)10.1076 +/- 0.0010
b (Angstrom)13.0403 +/- 0.0010
c (Angstrom)20.6260 +/- 0.0015
alpha (°)84.364 +/- 0.005
beta (°)82.811 +/- 0.004
gamma (°)76.492 +/- 0.004
Volume (A**3)2615.9 +/- 0.4
Mosaicity (°)1.820 +/- 0.004

Data collection

Summary

Total number of images collected327
Total exposure time109.1 minutes
Data collection exposure time108.0 minutes
Data collection wall-clock time122.2 minutes

Experimental Conditions

Wavelength0.71073 A
Crystal to detector distance36.00 mm

Scans

TypeName# imagesTotal
Rotation		Per frame
Rotation		Exposure
per frame		Used in
scaling
data collections01f181362.0° phi2.000°20 secondsYes
data collections02f13 26.0° omega2.000°20 secondsYes
data collections03f28 56.0° omega2.000°20 secondsYes
data collections04f28 56.0° omega2.000°20 secondsYes
data collections05f28 56.0° omega2.000°20 secondsYes
data collections06f13 26.0° omega2.000°20 secondsYes
data collections07f28 56.0° omega2.000°20 secondsYes
Phi/Chii01f - i08f88 seconds

Scalepack Scaling

Deleted observations

Rejected   2
Zero sigma or profile test  18
Overload or incomplete profile1306
Sigma cutoff 520
High resolution limit  93

Final Data Set

Scale factor10.00
Number of 'full' reflections   973
Number of 'partial' reflections 35402
Total number of integrated reflections 10799
Total number of unique reflections  7204
Data completeness  59.2%
Resolution range7.00-0.77 A
Theta range2.91°-27.48°
Average Intensity   70.3
Average Sigma(I)    3.6
Overall R-merge (linear)  0.156

Sadabs Results

Parameter refinement on 30032 reflections reduced R(int) from 0.1230 to 0.0701

Before rejection, 40698 reflections total and 12226 unique

After rejection, 35617 reflections total and 12084 unique

Runs

  Run 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1   15.9  0.0604   0.655 - 0.910   0.968 - 1.154   2.116   20624   15637
    2   15.4  0.0938   0.554 - 0.597   0.990 - 1.092   1.997    1098     784
    3   15.4  0.0620   1.153 - 1.240   0.967 - 1.081   2.094    3171    2434
    4   15.4  0.0902   1.247 - 1.558   0.993 - 1.077   2.127    3102    2281
    5   15.4  0.0630   1.279 - 1.369   0.990 - 1.110   2.077    3175    2395
    6   15.4  0.0883   0.569 - 0.602   0.972 - 1.128   2.199    1281     961
    7   15.4  0.0679   1.086 - 1.384   0.966 - 1.097   2.195    3166    2251
Ratio of minimum to maximum apparent transmission: 0.837756

Metadata

  Group    Service  
  Operator   Peter Horton  
  Sample Owner   Dr MA Beckett  
  Local Code   MAB/JT/23  
  Formula   C19 H22 B5 O10 P1  
  Crystal Colour    Colourless  
  Crystal Habit   Cut Block  
  Crystal Size   0.2 x 0.13 x 0.07 (mm3) 
  Temperature   120(K) 
  Generator   50 (kV)   85 (mA) 
  Primary Solvent     
  Other Solvents     

File Explanations

SampleCode.zip
      SampleCode.hkl - data corrected using  SADABS
      SampleCode_merge_none.hkl - equivalents and friedels kept separate  (See "Final Data Set" table in this report)
      SampleCode.p4p - skeleton p4p file for use with XPREP
      SampleCode.htm - this summary file

Southampton CIF entry fields

_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type   'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method          '\f & \w scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'

_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 

Software References

Unit Cell Determination using DirAx:
Duisenberg AJM. Indexing in Single-Crystal Diffractometry with an Obstinate List of Reflections. Journal of Applied Crystallography 1992; 25: 92-96.
Duisenberg AJM, Hooft RWW, Schreurs AMM, Kroon J. Accurate cells from area-detector images. Journal of Applied Crystallography 2000; 33: 893-898.

Diffractometer control and strategy calculation using COLLECT:
Hooft RWW. COLLECT data collection software, Nonius B.V., 1998.

Standard Data Reduction using HKL(Denzo & Scalepack):
Otwinowski Z, Minor W. Processing of X-ray diffraction data collected in oscillation mode. Macromolecular Crystallography, Pt A. 1997; 276: 307-326.

Absorption Correction
Sheldrick, G. M. (2007). SADABS. Version 2007/2. Bruker AXS Inc., Madison, Wisconsin, USA.

Non-Standard Data Reduction using EvalCCD:
Duisenberg AJM, Kroon-Batenburg LMJ, Schreurs AMM. An intensity evaluation method: EVAL-14. Journal of Applied Crystallography 2003; 36: 220-229.

For more information visit the service web site at: http://www.soton.ac.uk/~xservice/